The primary objective of this research is to elucidate the interactions, mechanisms and biochemistry of the spider silk producing process at the molecular level. Our primary focus is to characterize the protein-rich fluid in the various spider silk producing glands. We have been using a battery of magnetic resonance methods including solution and solid-state nuclear magnetic resonance NMR and micro imaging MRI in combination with wide angle and small angle X-ray diffraction WAXD and SAXD techniques at Argonne National Laboratory ANL to probe silk protein structure and dynamics prior to and following fiber formation. We have established a number of methods for isotopically 2H13C15N enriching the silk proteins during the course of our AFOSR funding that have allowed us to investigate the structure, dynamics, and organization of spider silk protein within the silk gland and in the final spun fiber with a range of magnetic resonance methods. We successfully developed magnetic resonance imaging MRI techniques with localized spectroscopy to probe the silk glands of spiders and map protein structure through out the silk gland.